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WO2005001920A1 - Procede de generation de plasma, procede de nettoyage et procede de traitement d'un substrat - Google Patents

Procede de generation de plasma, procede de nettoyage et procede de traitement d'un substrat Download PDF

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Publication number
WO2005001920A1
WO2005001920A1 PCT/JP2004/009026 JP2004009026W WO2005001920A1 WO 2005001920 A1 WO2005001920 A1 WO 2005001920A1 JP 2004009026 W JP2004009026 W JP 2004009026W WO 2005001920 A1 WO2005001920 A1 WO 2005001920A1
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WO
WIPO (PCT)
Prior art keywords
gas
plasma
mixed gas
cleaning
pressure
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2004/009026
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English (en)
Japanese (ja)
Inventor
Hiroshi Kannan
Noboru Tamura
Kazuya Dobashi
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Tokyo Electron Ltd
Original Assignee
Tokyo Electron Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2003185160A external-priority patent/JP4558284B2/ja
Priority claimed from JP2003185161A external-priority patent/JP4558285B2/ja
Application filed by Tokyo Electron Ltd filed Critical Tokyo Electron Ltd
Priority to US10/562,400 priority Critical patent/US20060226119A1/en
Publication of WO2005001920A1 publication Critical patent/WO2005001920A1/fr
Anticipated expiration legal-status Critical
Priority to US12/752,813 priority patent/US8574448B2/en
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32082—Radio frequency generated discharge
    • H01J37/321—Radio frequency generated discharge the radio frequency energy being inductively coupled to the plasma
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/3065—Plasma etching; Reactive-ion etching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32357—Generation remote from the workpiece, e.g. down-stream
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/311—Etching the insulating layers by chemical or physical means
    • H01L21/31105—Etching inorganic layers
    • H01L21/31111—Etching inorganic layers by chemical means
    • H01L21/31116—Etching inorganic layers by chemical means by dry-etching

Definitions

  • the present invention generally relates to a method for manufacturing a semiconductor device, and more particularly to a cleaning method using plasma and a substrate processing method.
  • the present invention also relates to a plasma generator, and more particularly to a plasma ignition method.
  • Plasma generators are widely used in the manufacture of semiconductor devices and liquid crystal display devices. For example, by using a plasma generator, it is possible to perform a film forming process or an etching process at a low temperature at which the concentration distribution of impurity elements formed in a semiconductor substrate does not change. Also, the plasma generator is used to clean the inside of the processing container after performing the substrate processing.
  • FIG. 1 shows the configuration of a typical conventional single-wafer CVD apparatus 10.
  • a single-wafer CVD apparatus 10 includes a susceptor 12 that includes a heating mechanism (not shown) and holds a substrate 12A to be processed, and uses a vacuum pump 13 to shut off a valve 13A and conductance valve 13B.
  • the processing vessel 11 includes a processing head 11 that is evacuated through the susceptor 12 and a shower head 14 that is supplied with a raw material gas from a raw gas supply system 15 via a line L1 and a valve VI. It is provided so as to face the substrate to be processed 12A.
  • the source gas supply system 15 includes source gas sources 15A to 15C.
  • the source gas in the source gas source 15A is connected to the line L1 via a valve 15VA, and the source gas in the source gas source 15B is the source gas.
  • the source gas in the source gas source 15C is supplied to the line L1 via a valve 15VB, and the source gas is supplied to the line L1 via a valve 15VC.
  • the raw material gas supplied through the line L1 is released into the process space in the processing container 11 via the shower head 14, and is subjected to a decomposition reaction on the surface of the processing target substrate 12A, thereby causing the processing target substrate 12A to degrade.
  • a desired film is formed on the surface of the substrate 12.
  • a lube structure is provided for taking in and out the substrate to be processed 12A, and the glove structure is connected to a substrate transfer chamber.
  • the single-wafer CVD apparatus 10 constitutes a single-wafer substrate processing system together with another processing apparatus coupled to the substrate transfer chamber.
  • the substrate temperature is controlled by a heating device formed in the susceptor 12 during the film forming process. Is kept at a relatively low temperature, for example, at about room temperature to about 150 ° C. (cold wall).
  • a cleaning module 16 including an etching gas source 16 A, a plasma gas source 16 B, and a remote plasma source 16 C is provided outside the processing vessel 11.
  • the highly reactive etching gas formed by the 16C is emptied into the process space inside the processing vessel 11 via the line L2 and the valve 16V.
  • the etching gas source 16A is an etching containing fluorine such as NF.
  • Gas is supplied to the remote plasma source 16C via a valve 16VA and the plasma
  • the magaz source 16B supplies a rare gas such as Ar to the remote plasma source 16C via a valve 16VB.
  • the cleaning gas containing fluorine includes halogen compound such as NF.
  • non-halogenated compounds such as CH COOH may be used.
  • the plasma may be any organic compound.
  • non-halogenated compounds such as CH COOH may be used.
  • the plasma may be any organic compound.
  • He, Ne, Kr, Xe, etc. may be used as the diluent gas from the gas source 16B, and H ⁇ , O, H, N, CF, etc. may be used as the diluent gas in addition to the rare gas.
  • Such a remote plasma source 16C includes an inductively coupled (ICP) plasma generator 20 shown in Fig. 2A, an electron cyclotron resonance (ECR) plasma generator 30 shown in Fig. 2B, and a helicon plasma generator shown in Fig. 2C.
  • ICP inductively coupled
  • ECR electron cyclotron resonance
  • a helicon plasma generator shown in Fig. 2C.
  • a wave excitation type plasma generator 40, a microwave resonator type plasma generator 50 shown in FIG. 2D, a toroidal type plasma generator 60 shown in FIG. 2E, and the like are known.
  • a parallel plate (CCP) type plasma generator 70 shown in FIG. 3 is used as a plasma source provided inside the processing vessel 11.
  • a high-frequency coil 22 is wound around a plasma container 21 in which plasma is generated, and is driven by a high-frequency power supply 23, so that the inside of the plasma container is To form a plasma.
  • a magnetic field is applied by disposing a magnet 32 around the plasma container 31 in a space inside the plasma container 31 in which plasma is generated. Further, in this state, by supplying a microwave from the microwave power supply 33 to the gas inside the container 31, electron cyclotron resonance is induced in the gas inside the container 31.
  • a magnet 44 is provided in proximity to a plasma container 41 in which plasma is generated, and a loop antenna 42 is provided in proximity to the plasma container 41.
  • This loop antenna is driven by high-frequency power from the high-frequency power supply 43, and a high-density plasma is formed by propagating a recombination wave into the plasma container 41.
  • a plasma container 51 in which plasma is formed forms a microwave resonator.
  • Plasma is formed by driving a microwave from the wave power supply 52 by an electric field.
  • a circulating gas passage 61 provided with a gas inlet 61A and a gas outlet 61B is provided, and a high-frequency coil is provided outside the gas passage 61. 62 is wound.
  • the rare gas such as Ar introduced into the gas inlet 61A circulates in the circulating gas passage 61.
  • the high-frequency coil 62 is driven by microwaves, so that the rare gas Is induced in the plasma.
  • a pair of parallel plate electrodes 71A and 71B are arranged in a plasma container 71 in which plasma is generated.
  • the plasma generator 70 in FIG. 3 itself constitutes a plasma processing apparatus, and the plasma container 71 is used as a processing container.
  • the lower electrode 71B serves as a susceptor, on which the substrate to be processed is mounted.
  • the plasma is generated away from the wall surface of the generator, and a preferable feature is that the introduction of large-mass charged particles such as ions into the process space inside the processing chamber 11 is small. Therefore, it is considered that the plasma processing apparatus 10 of FIG. 1 is preferably used as a powerful toroidal type plasma generator remote plasma source 16C.
  • FIG. 4 shows in more detail the toroidal plasma generator 60 shown in FIG. 2E used as the remote plasma source 16C.
  • the plasma generator 60 has a circulating gas passage 61 provided with a gas inlet 61A and a gas outlet 61B, and a high-frequency coil 62 is provided outside the gas passage. It is wound.
  • the rare gas such as Ar introduced into the gas inlet 61A circulates in the circulating gas passage 61.
  • the high-frequency coil 62 is driven by high-frequency electric power, so that the rare gas To induce plasma.
  • a circulating current path indicated by a solid line 61a in FIG. 4 is formed in the gas passage 61, and the high-frequency coil Fig. 4 The path is narrowed down to a path corresponding to the current path 61a as shown by a broken line 61b in the middle.
  • the plasma generator 60 of FIG. 4 since the high-density plasma is formed at a position distant from the wall defining the circulating gas passage 61, the plasma is accelerated particularly by high energy. It is possible to form plasma with less contamination by less sputtering of wall surfaces by electrons. In addition, the plasma is maintained stably without such contamination.
  • Patent Document 1 U.S. Patent No. 6374831
  • the toroidal type plasma generator 60 shown in FIG. 4 once a high-density plasma is formed, the force that can stably maintain it is understood from the above description. There is a problem with ignition. This problem is particularly prominent when, for example, the plasma generator 60 of FIG. 4 is used as the remote plasma source 16C in the CVD apparatus 10 of FIG.
  • the NF etching gas is used for etching the power NF supplied to the remote plasma source 16 C and the etching of F, CF, CF, CF, SF, C1F, and the like.
  • the fluorine-containing compound used has an ionization energy much larger than that of Ar. Therefore, in the remote plasma source 16C, the Ar gas from the Ar gas source 16B contains fluorine such as NF containing F having a high electronegativity in the Ar gas from the Ar gas source 16B. If the contained etching gas is added, there arises a problem that it is difficult to ignite the plasma in the remote plasma source 16C.
  • FIG. 5 shows that the inventor of the present invention used the toroidal type apparatus 60 of FIG. 4 as the remote plasma source 16 C in the CVD apparatus 10 of FIG.
  • the pressure in the circulating gas passage 61 of FIG. 4 was set to 1333 Pa (l OTorr)
  • the temperature of the susceptor 12 was set to 100 ° C.
  • the total flow rate of Ar gas and NF gas was
  • Etching (cleaning) of the thermal oxide film formed on the substrate 12A of FIG. 1 is performed under the condition of 1500 SCCM.
  • the vertical axis indicates the cleaning rate of the thermal oxide film per minute.
  • the remote plasma source 16C is driven by a high frequency of 400 kHz.
  • the cleaning rate increases as the NF gas concentration in the Ar / NF mixed gas increases.
  • FIG. 6 shows the relationship between the cleaning speed and the NF gas partial pressure in the CVD apparatus 10 of FIG.
  • the experiment shown in FIG. 6 was also conducted by the inventor of the present invention in the research on which the present invention was based, and the toroidal plasma generator 60 shown in FIG. 4 was used as the remote plasma source 16C.
  • the concentration of the NF gas supplied to the remote plasma source 16C was set to 45% and the total flow rate of the Ar / NF mixed gas was set to 1500 SCCM, The etching of the thermal oxide film is performed while changing the total pressure in the processing vessel 11.
  • the concentration of the NF gas when the concentration of the NF gas is fixed, the total pressure in the processing vessel 11 (accordingly, the partial pressure of the NF gas) is increased to increase the etching rate of the thermal oxide film, that is, It can be seen that the tallying speed increases. From the relationship in Fig. 6, it can be seen that when the NF concentration is set to 45%, a cleaning rate (etching rate) exceeding 500 nm / min is realized at a pressure of about 266 Pa (2 Torr) or more.
  • FIGS. 5 and 6 are supplied to the remote plasma source 16C when the toroidal plasma generator 60 shown in FIG. 4 is used as the remote plasma source 16C in the CVD apparatus 10 of FIG. It is shown that by increasing the NF gas concentration or partial pressure in the Ar / NF mixed gas, a cleaning speed exceeding 500 nm per minute can be achieved.Therefore, in order to efficiently perform cleaning in the CVD apparatus 10 in FIG. Thus, NF gas concentration It is understood that it is preferable to increase the degree.
  • FIG. 7 shows the relationship between the plasma sustaining power in the toroidal plasma generator 60 of FIG. 4 and the NF concentration in the Ar / NF mixed gas supplied to the plasma generator 60.
  • FIG. 8 shows the relationship between the plasma maintenance power in the toroidal plasma generator 60 of FIG. 4 and the total pressure of the Ar / NF mixed gas supplied to the plasma generator 60.
  • Plasma is generated under the condition that the total flow rate is set to 1500 SCCM.
  • the plasma maintenance power in the Ar / NF mixed gas decreases in total pressure.
  • the plasma when the total pressure is about 333 Pa (2.5 Torr), for example, the plasma is maintained at a high frequency power of about 3 kW. On the other hand, when the total pressure is about 2000 Pa (15 Torr), it can be seen that the plasma cannot be maintained unless the RF power exceeding 4 kW is applied.
  • toroidal plasma generators especially those with electronegativity such as NF,
  • the plasma is no longer ignited just by being burned. When the total pressure rises, the plasma ignites No longer.
  • the problem is that the plasma sustaining power and NF concentration or partial pressure in Figs.
  • the plasma cannot be ignited unless the NF gas is removed by sufficiently purging the circulating gas passage 61 in FIG. 4 at the time of plasma ignition.
  • the plasma generating apparatus of either type shown in FIGS. 2A to 2F or FIG.
  • a high drive voltage must be applied.However, if such a high drive voltage is applied, the coils and electrodes are immediately turned on when the plasma is ignited.
  • the impedance of the driving system including the driving system greatly changes, and the overshoot driving voltage may damage the driving system and the high-frequency power supply.
  • Another object of the present invention is to provide a toroidal plasma generator, a plasma ignition method for igniting plasma with respect to a mixed gas of Ar gas and NF gas, and a substrate treatment using such a toroidal plasma generator. It is to provide a method.
  • Another object of the present invention is to provide a plasma cleaning method capable of igniting plasma at a low voltage and thereby avoiding damage to a power supply, a coil, an electrode, and the like due to a high voltage.
  • the present invention provides
  • a gas passage having a gas inlet and a gas outlet, forming a peripheral circuit
  • a toroidal-type plasma generator having a coil wound around a part of the gas passage
  • the present invention also provides
  • a gas passage having a gas inlet and a gas outlet, forming a peripheral circuit
  • a toroidal-type plasma generator having a coil wound around a part of the gas passage
  • the present invention provides a plasma generation method characterized in that the plasma ignition step is performed under a total pressure of 6.65 to 66.5 Pa.
  • the present invention also provides
  • a method for cleaning a processing vessel exhausted by an exhaust system and coupled to a remote plasma source comprising:
  • the remote plasma source includes a gas inlet and a gas outlet, and includes a toroidal plasma generator having a gas passage forming a peripheral circuit, and a coil wound around a part of the gas passage.
  • the cleaning method includes the steps of: forming a radical containing F in the remote plasma source;
  • the cleaning step provides a cleaning method, wherein the inside of the processing container is tallied at the second pressure.
  • the present invention also provides
  • a method for processing a substrate in a processing vessel exhausted by an exhaust system and coupled with a remote plasma source comprising:
  • the remote plasma source includes a gas inlet and a gas outlet, and includes a toroidal plasma generator having a gas passage forming a peripheral circuit, and a coil wound around a part of the gas passage.
  • Etch NF or F at a concentration of at least 5% in Ar gas in the gas passage
  • the etching process is performed at the second pressure, and a substrate processing method is provided.
  • the present invention also provides
  • a cleaning method for cleaning the inside of a processing container in a first pressure band with radicals of a cleaning gas excited by plasma comprising:
  • a mixed gas of a dilution gas and a cleaning gas is supplied to the plasma generator from the first pressure zone.
  • a second pressure zone which is lower in temperature, to ignite the plasma,
  • a cleaning method characterized by including a step of increasing a pressure inside the processing container from the second pressure zone to the first pressure zone.
  • the present invention also provides
  • a substrate processing method for etching a surface of a substrate to be processed in a processing chamber in a first pressure zone by a plasma-excited etching radical for etching a surface of a substrate to be processed in a processing chamber in a first pressure zone by a plasma-excited etching radical.
  • the present invention provides a substrate processing method including a step of increasing a pressure inside the processing container from the second pressure zone to the first pressure zone.
  • the present invention provides
  • a cleaning method for cleaning the inside of a processing container in a first pressure band with radicals of a cleaning gas excited by plasma comprising:
  • the present invention provides
  • a mixed gas of Ar gas and NF gas containing at least 5% of NF is supplied into the gas passage, and 6.6 is supplied by high frequency power.
  • the throughput of cleaning and substrate processing can be greatly improved. Also, once the plasma is ignited, it is possible to shift from the plasma ignition point to the process point where tally jung and etching are performed without extinguishing the plasma, making it possible to execute an efficient plasma process Become.
  • the present invention by reducing the gas pressure at the time of plasma ignition, it becomes possible to perform plasma ignition at a low voltage even with a gas containing a halogen compound. As a result, the occurrence of a large voltage overshoot caused by a large impedance change at the moment of plasma ignition and the damage to the drive power supply, electrodes, coils, etc. due to this are avoided.
  • the desired cleaning process or etching process can be efficiently performed by increasing the gas pressure to a predetermined process condition while maintaining the plasma. Become.
  • the plasma is ignited with respect to the gas containing the halogenated compound, especially in the case of frequently interrupting the plasma, such as in a single-wafer processing step, the plasma is ignited every time the plasma is ignited. This eliminates the need for purging the gas containing the halogenated compound, thereby greatly improving the throughput of the tallying or substrate processing.
  • FIG. 1 is a diagram showing a configuration of a CVD apparatus to which the present invention is applied.
  • FIG. 2A is a diagram showing an outline of a conventional inductively coupled plasma generator.
  • FIG. 2B is a diagram showing an outline of a conventional electron cyclotron resonance type plasma generator.
  • FIG. 2C is a diagram showing an outline of a conventional helicon wave excitation type plasma generator.
  • FIG. 2D is a diagram showing an outline of a conventional microwave resonator type plasma generator.
  • FIG. 2E is a diagram showing an outline of a conventional toroidal plasma generator.
  • FIG. 3 is a diagram showing an outline of a conventional parallel plate type plasma generator.
  • FIG. 4 is a view showing a configuration of a conventional toroidal plasma generator used in the CVD apparatus of FIG. 1.
  • FIG. 5 is a graph showing the relationship between the NF3 concentration in the Ar / NF mixed gas used in the plasma cleaning process and the tallying speed.
  • FIG. 6 is a diagram showing the relationship between the total pressure of an Ar / NF mixed gas used in the plasma cleaning process and the tallying speed.
  • FIG. 7 is a graph showing a relationship between NF concentration and plasma maintenance power in an Ar / NF mixed gas used in a plasma cleaning process.
  • FIG. 8 is a diagram showing the relationship between the total pressure of an Ar / NF mixed gas used in the plasma cleaning process and the plasma maintenance power.
  • FIG. 9 is a diagram for explaining a search for plasma ignition conditions according to the first embodiment of the present invention.
  • FIG. 10 is a diagram showing plasma ignition conditions found according to the first example of the present invention.
  • FIG. 11 is a diagram showing the relationship between the plasma ignition voltage and the total pressure found by the first embodiment of the present invention.
  • FIG. 12 is a view showing plasma ignition conditions of Ar / F gas according to a second embodiment of the present invention.
  • FIG. 13 is a diagram showing a transition from a plasma ignition point to a plasma cleaning or plasma etching process point according to a third embodiment of the present invention.
  • FIG. 14 is a view showing a configuration of a gas flow rate switching mechanism used in a third embodiment of the present invention.
  • FIG. 15 is a view showing a gas and RF power supply sequence in a plasma cleaning / etching step according to a third embodiment of the present invention.
  • Microwave resonator type plasma generator Microwave resonator
  • the toroidal plasma generator has a preferable feature that contamination in the substrate processing step using plasma is small because sputtering of the plasma generator wall by plasma is suppressed.
  • plasma ignition is difficult and plasma ignition is to be performed, it is necessary to eliminate the etching gas or cleaning gas containing halogen with a high electronegativity such as NF and perform ignition in an atmosphere of 100% Ar gas. was there.
  • FIG. 9 shows that, based on such an idea, the inventor of the present invention conducted a study on the basis of the present invention to obtain a toroidal plasma generator 60 (ASTRONi, MKS, US Pat. No. 150628), the plasma ignition conditions were changed in the Ar / NF mixed gas.
  • the total pressure and flow rate of the Ar / NF mixed gas and the NF concentration in the mixed gas are determined.
  • the plasma ignition point was searched with various changes, the results shown in Fig. 10 were obtained.
  • a high frequency of 400 kHz is supplied at a power of 1500 W.
  • FIG. 10 shows that the NF was reduced by reducing the total pressure in the gas passage 61 at the time of plasma ignition to 66.5 Pa (0.5 Torr) or less, preferably 6.65 Pa (0.05 Torr) or less. It can be seen that plasma ignition is possible in an Ar / NF mixed gas containing 5% or more, and in particular, even if the NF concentration in the Ar / NF mixed gas reaches 45%, plasma ignition may be possible. .
  • FIG. 10 is a view showing a state in which A is supplied to the toroidal type plasma generator at the time of plasma ignition.
  • the force range is limited, as the gas flow rate is reduced to 20 SCCM, 5 SCCM, and 3 SCCM, the NF concentration range and pressure range where plasma ignition occurs expands.
  • the gas flow rate of the Ar / NF mixed gas was 100SCC.
  • FIG. 11 shows the relationship between the plasma ignition voltage and the total pressure in the toroidal plasma generator 60 of FIG. 4, which was obtained based on the results of FIGS.
  • the NF power% is contained in the Ar / NF mixed gas.
  • the plasma ignition voltage decreases as the total pressure decreases, and reaches a minimum at a pressure approximately corresponding to the ignition point indicated by ⁇ in FIG. If the pressure decreases below this, the collision probability decreases, and as a result, the plasma ignition voltage sharply increases.
  • the NF is 5
  • FIG. 12 shows that the inventor of the present invention uses a mixed gas of Ar and F in the gas passage 61 in the toroidal plasma generator 60 shown in FIG. 4 at various F concentrations (F / (Ar + F)).
  • F / (Ar + F) various F concentrations
  • the flow rate of the Ar / F mixed gas was set to 100 SCCM, and a high frequency of OO kHz was supplied at a power of 1300 W.
  • plasma ignition is about 6.65 Pa (0.05 Torr) or more and 66.5 Pa when the F concentration in the mixed gas is 5%.
  • the inventors of the present invention found that, in the research on which the present invention is based, the Ar gas contains a halogen with a high electronegativity such as NF or F in the toroidal plasma generator as shown in FIG. We succeeded in finding out that plasma ignition was possible and the conditions under which plasma ignition was possible even when a mixed gas containing gas was supplied.
  • a halogen with a high electronegativity such as NF or F
  • the pressure or gas flow actually used for cleaning or etching in the CVD apparatus is much larger than the ignition point shown in FIG. In 60, after the plasma is ignited at the ignition point in Fig. 9 or 10, it is required that the conditions can be changed to the process point where the process is actually performed without extinguishing the plasma.
  • the concentration of NF in the ArZNF mixed gas becomes 50% or more, and the pressure (total pressure) also increases. 13
  • the inventors of the present invention set the ignition point corresponding to the plasma ignition point described with reference to Fig. 9 or 10 for the CVD apparatus 10 shown in Fig. 1 as shown in Fig. 13. From point (1), the actual cleaning or Up to the process point (2), the total pressure and flow rate of the Ar / NF mixed gas were changed in various ways, and it was verified whether the plasma was maintained from the point (1) to the point (2). However, in this experiment, the valve 16Vc was fully opened in the CVD apparatus 10 of FIG. 1, and the pressure in the gas passage 21 of the toroidal type plasma generator 20 of FIG. Inside the pressure is substantially equal.
  • the total pressure at the ignition point (1) was set to about 11 Pa (0.08 Torr), and the total flow rate of the Ar / NF mixed gas was set to 3 SCCM, and the process point (2) , The total pressure is set to 1330 Pa (10 Torr), and the total flow rate of the ArZNF mixed gas is set to 3 SLM.
  • the gas flow rate is increased from the ignition point (1) while maintaining the pressure of about 11 Pa (0.08 Torr), and reaches the point (4). That is, from point (1) to point (4), in the CVD apparatus 10 of FIG. 1, the pressure in the processing vessel 11 is maintained constant even if the flow rate of the Ar / NF mixed gas increases.
  • the conductance valve 13B of the exhaust system is gradually opened, and at the point (4), the conductance valve 13B is fully opened.
  • the point (4) is determined by the capacity of the conductance valve 13B and the vacuum pump 13 cooperating therewith.
  • the conductance valve 13B is gradually closed while the flow rate of the Ar / NF mixed gas is kept constant, so that the pressure inside the processing vessel 11 and, accordingly, the gas passage 61
  • the total pressure inside gradually increases and reaches point (6) in the fully closed state. That is, the point (6) is determined by the gas leak amount and the capacity of the vacuum pump 13 when the conductance valve 13B is fully closed.
  • the flow rate of the Ar / NF mixed gas is increased while the conductance valve 13B is kept in the fully closed state, thereby obtaining the processing vessel 1
  • the flow rate of the ArZNF mixed gas is set to a predetermined value while maintaining the opening of the conductance valve 13B.
  • the route from point (4) and point (6), and hence the route from point (4) to point (5), and the route from point (6) to point (7) The path is determined by the design of the conductance valve 13B of the CVD device used and the capacity of the vacuum pump 13. If the maximum conductance of the conductance valve 13B is increased or the capacity of the vacuum pump 13 is increased, the point ( The route from 4) to point (5) shifts to the high flow side. When the minimum conductance of the conductance valve 13B is reduced or the capacity of the vacuum pump 13 is reduced, the path from the point (6) to the point (7) shifts to the high pressure side.
  • the process point (2) can be set to any of the conditions described above with reference to FIG.
  • the toroidal plasma generator 20 is used as a remote plasma source 16 C, and the plasma of an insulating film such as a thermal oxide film or a CVD oxide film is placed in the processing vessel 11.
  • Etching, plasma etching of a metal film such as a W film or a Ti film, plasma etching of a conductive nitride film such as a TiN film, and plasma etching of a polysilicon film can be performed.
  • the NF gas source 16A is provided with a plurality of mass flow controllers 16a and 16b having different capacities as shown in FIG.
  • the Ar gas source 16B is also provided with a plurality of mass flow controllers 16c and 16d having different capacities, and these are switched by valves.
  • the mass flow controller 16a first increases the ArZNF3 mixed gas flow rate along the path C, and at the point (8) on the path C Considering a case where the mass flow controller 16a is switched to a larger capacity mass flow controller 16b, the flow rate is temporarily changed with the switching of the mass flow controller. And the force at which the total pressure may drop to point (9). Returning to point (10) on path C can be achieved by driving a larger mass flow controller 16b. At this time, according to the present embodiment, the plasma ignited at the point (1) will not be extinguished as long as the point (9) is located in the plasma maintaining region shown in FIG.
  • the point (10) after the return is not limited to the path C, but may be selected to an arbitrary point in the plasma maintenance region within a range where the flow rate is larger than that of the point (8). Can be.
  • the F concentration in the Ar / F mixed gas may be kept constant or may be changed during the pressurization.
  • the rare gas supplied into the plasma generator is not limited to Ar gas, and gases such as He, Ne, Kr, and Xe can also be used.
  • FIG. 15 shows a supply sequence of gas and RF power used in the cleaning or etching process according to the third embodiment of the present invention based on the above results.
  • a small amount of Ar gas and NF gas were supplied to the toroidal type plasma generator 60 of Fig. 4 and the total pressure of 6.65-66.5Pa (P1 ) Provide RF power below to ignite the plasma.
  • the pressure Pl in the ignition step and the flow rates of the Ar gas and the F gas at that time may be set so as to fall within the ignition range described with reference to FIG. [Fourth embodiment]
  • Fig. 11 The relationship shown in Fig. 11 above, that is, the tendency that the plasma ignition voltage decreases on the low pressure side and rapidly increases after passing the pressure corresponding to a certain minimum value is not limited to the toroidal type plasma generator, but is shown in Figs. In the plasma generators 20 to 70 described below, it is considered that the tendency is universally established regardless of the type of rare gas and the type of halogen-containing etching gas or cleaning gas.
  • the mixed gas of the rare gas and the gas containing the halogen compound may be mixed with the gas having the minimum ignition voltage shown in FIG. Ignition plasma using conditions
  • the cleaning / etching gas such as NF or F
  • the total pressure of the mixed gas of the rare gas and the cleaning Z etching gas is gradually increased to a desired process pressure according to the same sequence as in FIG. To increase.
  • the ignition point (1) corresponding to the pressure P1 of FIG. 15 is changed to the pressure P2 of FIG. 15 where the actual cleaning process is performed.
  • the total pressure and the gas flow rate can be achieved without extinguishing.
  • the route from point (4) to point (6) and therefore the route from point (4) to point (5), and the route from point (6) to point (7).
  • the path is determined by the design of the conductance valve 13B of the CVD apparatus used and the capacity of the vacuum pump 13.
  • the point ( The route from 4) to point (5) shifts toward the higher flow rate.
  • the minimum conductance of the conductance valve 13B is reduced or the capacity of the vacuum pump 13 is reduced, the path from the point (6) to the point (7) shifts to the high pressure side.
  • the process point (2) can be set to a known condition or deviation under which plasma cleaning can be efficiently performed.
  • cleaning in the CVD apparatus 10 of FIG. 1 is started from the time when plasma ignition occurs in the toroidal type plasma generator 20 used as the remote plasma source 16C.
  • the mixture ratio of Ar gas and NF gas in the Ar / NF mixed gas may be fixed or changed. ,.
  • the NF concentration in the Ar / NF mixed gas is increased during the transition from the ignition point (1) to the process point (2). In addition to this, it is possible to reduce it as necessary.
  • any one of the plasma generating apparatuses of FIGS. 2A to 2E is used as a remote plasma source 16 C, and a thermal oxide film or a CVD oxide film is formed in the processing chamber 11.
  • plasma etching of an insulating film plasma etching of an insulating film, plasma etching of a metal film such as a W film or a Ti film, plasma etching of a conductive nitride film such as a TiN film, and plasma etching of a polysilicon film can be performed.
  • the Ar gas source 16B is also provided with a plurality of mass flow controllers 16c and 16d having different capacities, and these are switched by using valves.
  • the Ar / NF mixed gas flow rate is first increased from the ignition point (1) in Fig. 13 by the mass flow controller 16a along the path C, and the point (8) on the path C Considering the case where the mass flow controller 16a is switched to the larger capacity mass flow controller 16b, the flow rate and total pressure may temporarily drop to the point (9) with the switching of the mass flow controller.
  • the mass flow controller 16b By driving the mass flow controller 16b with a certain force, it is possible to return to the point (10) on the route C.
  • the plasma ignited at the point (1) does not disappear.
  • the point (10) after the return is not limited to the path C, but may be selected to an arbitrary point in the plasma maintenance region within a range where the flow rate is larger than that of the point (8). Can be.
  • the present invention has been described above mainly on the case where the plasma is formed by supplying an Ar / NF mixed gas or an Ar / F mixed gas to a toroidal plasma generator.
  • the apparatus is not limited to the toroidal type plasma generator, and the present invention can be applied to the other plasma generators shown in FIGS. 2A to 2E or 3 as described in the fourth embodiment.
  • the diluent gas supplied for plasma formation is not limited to Ar.
  • the present invention relates to rare gases such as He, Ne, Kr, and Xe, or H ⁇ , ⁇ , H, N , CF and so on.
  • the cleaning / etching gas used in the present invention is not limited to NF or F, and it is also possible to use other halogen compound gas, and also a compound containing CH COO group such as CH COOH.

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Abstract

L'invention a trait à un procédé permettant de générer un plasma, dans un générateur de plasma toroïdal qui possède un passage doté d'un orifice d'admission de gaz et d'un orifice de sortie de gaz et formant un circuit, et une bobine enroulée autour d'une partie du passage de gaz. Le procédé selon l'invention est caractérisé en ce qu'il comprend une étape consistant à fournir un gaz mélangé constitué d'une part d'Ar contenant au moins 5 % de NF3 et d'autre part de gaz NF3, et à exciter la bobine à l'aide d'une puissance électrique haute fréquence, afin de provoquer l'ignition du plasma, l'étape d'ignition du plasma étant exécutée à une pression totale comprise entre 6,65 et 66,5 Pa.
PCT/JP2004/009026 2003-06-27 2004-06-25 Procede de generation de plasma, procede de nettoyage et procede de traitement d'un substrat Ceased WO2005001920A1 (fr)

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US8574448B2 (en) 2013-11-05
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US20060226119A1 (en) 2006-10-12
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